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Validation Including Uncertainty Estimation of a GC–MS/MS Method for Determination of Selected Halogenated Priority Substances in Fish Using Rapid and Efficient Lipid Removing Sample Preparation

Water Research Institute, Slovak National Water Reference Laboratory, Nábrežie arm. gen. L. Svobodu 5, 812 49 Bratislava, Slovak Republic
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Foods 2019, 8(3), 101; https://doi.org/10.3390/foods8030101
Received: 20 February 2019 / Revised: 12 March 2019 / Accepted: 13 March 2019 / Published: 18 March 2019
(This article belongs to the Special Issue Rapid Methods for Assessing Food Safety and Quality)
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Abstract

A rapid method is proposed for the determination of selected H2SO4 stable organic compounds—eight organochlorines (OCs; hexachloro-1,3-butadiene, pentachlorobenzene, hexachlorobenzene, hexachlorocyclohexane—HCH—isomers, heptachlor) and six polybrominated diphenyl ethers (PBDEs; BDE-28, 47, 99, 100, 153, 154)—in fish samples. In the method, a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation using pH-tuned dispersive liquid–liquid microextraction (DLLME) and H2SO4 digestion fish extract clean-up is followed by gas chromatography–triple quadrupole tandem mass spectrometry (GC–QqQ-MS/MS) analysis. The method was validated in terms of linearity, limits of the method, recovery, accuracy, analysis of standard reference material (NIST SRM 1946), and estimation of combined uncertainty of the measurement (top-down approach). For validation, chub composite samples were used, and subsequently, the method was successfully applied to analysis of real samples of eight fish species. Finally, the method passed the analytical Eco-Scale evaluation as “an acceptable green analysis method”, and showed its advantages (simplicity, rapidity, low cost, high extract clean-up efficiency, good sensitivity) when compared to other reported QuEChERS based methods. View Full-Text
Keywords: QuEChERS; dispersive liquid–liquid microextraction; sulfuric acid treatment; gas chromatography; tandem mass spectrometry; priority substances; fish samples QuEChERS; dispersive liquid–liquid microextraction; sulfuric acid treatment; gas chromatography; tandem mass spectrometry; priority substances; fish samples
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).
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Nagyová, S.; Tölgyessy, P. Validation Including Uncertainty Estimation of a GC–MS/MS Method for Determination of Selected Halogenated Priority Substances in Fish Using Rapid and Efficient Lipid Removing Sample Preparation. Foods 2019, 8, 101.

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